Process and means for regulating the gas pressure in containers



Sept. 29, 1953 T. D. MORGAN PROCESS AND MEANS FOR REGULATING THE GAS PRESSURE IN CONTAINERS Original Filed Jan. 4, 1949 T I .3 VAC; I

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1 l7 REG- 1 I6 l8 9 22 l9 E v27 1 2 -23) 2 2::{ a I :3 24 3 I D 5 a s ZR V 7 INVENTOR. T. o. MORGAN ATTORNEYS Patented Sept. 29, 1953 UNET rnocsss AND MEANS FDRBEGULATlNG THE GAS PRESSURE IN CONTAINERS Thomas D. Morgan, Oak Ridge. Tenn, assig'iioi' to Phillips Petroleum Company, a corporation of Delaware Original application January 4, 1949; Serial No.

69,226; nowPatent No. 2,582,6't7, dated January 15,1952. Divided and this application August 3, 1951, Serial No. 240,244

8 Claims. I

This invention relates to methods of and means for regulating the gas pressure in containers. In one aspect it relates to combinations and s'ubcombinations of evacuating means, gas supply means, conduit means, pressure regulating valve means and/or restricted orifices for controlling as flow in a conduit. The invention also relates to methods of determining changes in the composition of a gas and apparatus for carrying out the method as claimed in the patent application mentioned in the following paragraph.

Claims relating to method and means for indicating changes in the composition of a gas and claims to the combination of a gas pressure regulating means and a specific ionization gauge means, and to the ionization gauge fna'ns per se, have been allowed in my copending application Serial No. 69,226, filed January 4 1949, now U. S, Patent 2,582,547 of January 15, 1952, which application is the parent application of which the present application is a division.

It has been observed that the sum of the ions in a mass spectnim varies from one gas to another This sum is proportional to the total number of positive ions formed when a gas is bombarded by low speed electrons.

Many complicated means have been proposed in prior art for determining when the composition of a gas, such as a stream of gaseous product coming from a process in a plant, changes in composition, in order to monitor the process by indicating that the process is continuing as planned. When the composition of the gas varies, the process involved is not operating properly, and changes are made to restore theoperation to normal. Prior art devices testing the stream of gas generally have relied on analysis of the gas by means of spectrographic analysis, chemical analysis, analysis by mass spectrometer, or some other relatively complicated and slow form of analysis.

The present invention gets away from such complicated and expensive means of. analysis by relying on the simple fact that each gas forms a different number of positive ions when hembarded under the same conditions by low speed electrons. The present invention also avoids indicating false changes in the composition oi the gas caused by irregular thermal cracking of the original gas into other gases by contact with the filament from which the low speed electrons are being supplied. This is avoided by means of a novel arrangement of the filament, grids and plate so that the gas entering the test apparatus is subjected to low speed electron bombardment and the current is set up in the positive ions of the gas between a first grid and the plate before 2 the gas passes through said first grid into contact with the heated filame'nt. The gas which has contacted the heated filament and become thermally cracked is removed from the system from the other side of the grid from the gas which is conducting the indicating current.

A principal object of this invention is to provide suitable methods of and suitable means for supplying gas to containers at a regulated pres sure.

One object of my invention is to provide an proved method of detecting and indicating differences in the composition of a gas.

Another object is to provide improved ap-' paratus for carrying out such a method.

Another object is to provide such a method and apparatus in which the positive ions conducting the current are bombarded by low speed electrons without coming in contact with any heated ele ment which would change their composition by thermal cracking of the like.

Another (abject is to provide an impr'cived method and means of detecting a difference in. the composition of the gas by measuring an ionization current in said gas in an improved .ionization tube.

Another object of the invention is to detect aiid indicate changes in the tube of a gas stream and thereby to qualitatively determine the gas causing the deviation from the indication given by a gas of standard composition.

Another object is to indicate changes iii the composition of a gas to provide a monitor which indicates when changes in a process of producing a gas should be made.

With a pure gas an object of the invention is to give an indication of the presence of impurities in said gas,

With binary mixtures of gases an object of the invention is to analyzethe mixture to determine the exact percentage of each gas present.

With mixtures of known gases an object of the invention is to analyze the mixture to determine the exact percentage of each gas present.

Another object is to provide an improved gas ionization tube which is rugged, simple in com position, is not effected by products of thermal cracking,- and which is relatively cheap and easy to operate. p g

Numerous other objects and advantages willbe apparent upon reading the accompanying specification, claims and drawings.

Figure 1- is an elevational view with parts in cross section of an ionisation tube and means to supply the same with a stream of gas to be tested embodying the present invention, along with a wiring diagram for the same.

Figure 2 is an elevational view of a similar system employing the same type of ionization tube but having a modified system for supplying gas.

In Figure 1 a device for indicating changes in the composition of a gas by ionization currents generally designated as 3 is attached to a pipe 4 containing a flowing stream of gas which passes out through pipe '5. A small amount of this gas is constantly being drawn into instrument 3 through pipe 1 under the control of a constant pressure regulating valve 8 which is designed to maintain the pressure in space 9 at a substantially constant pressure.

Also connected to apparatus 3 is an exhaust pipe H by which the interior of 3 is exhausted to a substantially constant pressure of approximately 10- mm. of mercury by means of any suitable vacuum pump l2. Vacuum pump I2 is regulated by constant pressure regulator [3 which may be of any usual type, regulator l3 being controlled as shown by the dotted lines between the pressure regulator i3 and tube H. Vacuum pump l2 discharges through line Hi to the atmosphere. In many installations with various types of vacuum pumps [2, it has been found that one pump alone does not provide a constant enough vacuum and it is customary to use separate pumps (not shown) in series in pipe M with pump l2. For example, pump I2 could be a VMF-ZO oil diffusion pump and downstream in line 14 (not shown) and connected in series therewith a VMF-S oil diffusion pump and then a Welch duo seal fore pump. Also in line H before entering pump l2 an ice trap (not shown) may be provided. Chambers containing desiccant (not shown) could supplement the ice trap if the gas being tested contains water vapor. As such elaborations on vacuum pump l 2 are well known in the art of evacuating vessels it is not believed desirable to confuse the invention by elaborating on the type of vacuum pump system used at IE, it being understood that any suitable system known to the prior art for producing a vacuum in the neighborhood of 10* mm. of mercury which can be regulated to give a relatively constant pressure in tube 1 I is satisfactory in the practice of the present invention.

The pressure in the space 9 is of course considerably higher than 10- mm. of mercury because it is difficult to find a regulating valve 8 which is accurate at such a pressure; however, any system known to the prior art for getting the pressure in line 3 down to the desired pressure in space it may be employed. I prefer however r to employ a restricted orifice I! in a thickened portion N3 of tube 7 so that the pressure in space 9 may be in the neighborhood of 2 mm. of mercury while that in space I6 and space H is approximately 10 mm. of mercury. U

While other shapes of apparatus may be em ployed provided the principle of operation is the same, it is preferred to use as the ionization tube l9 of apparatus 3 a cylindrical tube preferably made of glass. A plate, 2| is provided inside the tube, which plate should have a considerable extent and preferably extends entirely around the tube to serve as the ion collector plate. I find the best way of forming this plate is to vaporize and depo it platinum on the glasssurface of tube l9. Metallic plate 2! is connected to wire 22. A source of negative electrons is provided and is shown in the form of a naked tungsten metal filament 23. Other metal filaments may be employed provided they are not poisoned by gases.

Obviously other types of heated cathodes may be employed, for example, the filament 23 may be sheathed in a porcelain tube (not shown) which porcelain tube is heated to incandescence and this porcelain tube may have metallic substances such as tungsten metal deposited thereon. However, it is not believed necessary to go into detail on the electron emissive cathode 23 as such cathodes are well known in the electron art and any type producing slow electrons is satisfactory. By slow electron I mean an electron having a velocity within the ranges understood by those skilled in the art which upon being accelerated by grid 24 would be suitable for causing the formation of positive ions in the gas in the pressure of 19- mm. of mercury. I have chosen a pressure of the magnitude of about 1() mm. of mercury because at that pressure positive ions are more easily and more uniformly formed by electron bombardment, but those skilled in the art can easily predict the amount this pressure can be changed without departing from the present invention, for as long as the same type of operation occurs the process is unchanged and the present invention is being employed.

Between the electron source 23 and the positive collection plate 21 I prefer a positive charged grid generally designated as 24. Grid 24 is preferably composed of two elements, the first being a helical wire 26 suitable for degassing the metallic parts of tube l9, as will be explained later, and a gauze wire cylinder 21 maintained at the same potential by wire 28. Tube 21 extends entirely around filament 23 but to avoid confusion, has not been drawn except where it is in section, as drawing all of the wires in cylinder 2! in back of filament 23 would make it almost impossible to see filament 23.

While the particular mode of supporting grid 21 is immaterial I prefer to imbed the lower end in an annular glass boss 29 formed in the wall of tube I9 and the upper end of 2'? is similarly imbedded in the lower end of tube 31 which forms an extension of tube II. It will be obvious that gas coming from I3 passes in space 32 between plate 2i and grid 21 before passing through grid 21 and out tube 3| and tube H, and it will also be obvious that any of the gas which contacts heated filament 23 and is thermally cracked thereby will pass up tube 3| without reaching plate 2|.

Th wiring diagram will now be explained. In order to have a reference point let us say that wire 33 is at an intermediate potential. Filament 23 is at the same potential at the top of the filament but there is a difference of about the magnitude of 5 volts provided by battery 34 and rheostat 36 between the ends of the filament which are connected to wires 31 and 33. Most of the current from battery 35 is forced to go through wires 3! and 38 by relatively high resistances 39 and 4|, which however allow wire 33 to be at the same average potential as filament 23.

Plate H is preferably maintained at a lower potential than filament 23, but this is not essential as long as plate 2| is at a considerably lower potential than grid 21 in order that positive ions created in the space between grid 21 and plate M will be urged toward plate 21 by electrostatic forces and will conduct a current thereby to plate 2!. As shown in the drawing it is preferred to provide a battery 42 which will keep plate 2! about 12 volts or so below the potential of filament 23 and about or volts below the potential of grid 21.

preferable to substitute one of the many constant current controls now on the market, as such an automatic electronic current control circuit (not shown) can do a better job of regulating the current in wire 41 to about milliamperes than man ual operation of rheostat 45.

The operation of Figure 2 is very similar except for the means of lowering the pressure from line 4 down to that necessary in tube N. In many plant operations the pressure in line 4 is too high to permit a single stage reduction of pressure by regulator 33, so in Figure 2 the pressure having been made constant by regulator 8 in pipe 53, a definite volume in pipe 62 of this gas under the pressure in pipe 53 is collected in pipe 62 by opening valve 51 and closing the same and then this gas is passed to storage vessel 64 at a low pressure by opening valve 59 and closing the same. The gas in vessel 64 is at a substantially uniform pressure during the cycles employing valves 57 and 59 and by the time this gas passes through orifice I! into chamber I!) it is at a substantially constant reduced pressure as desired.

It should be noted that after the gas passes through positively charged grid 21, it contacts heated filament 23 and is thereby cracked to form a different gas, that any positive ions formed in this different gas by electrons emitted from filament 23 cannot get through grid 2'! because they are repelled by the positive charge on the grid, and therefore they must pass up tube 33 and be exhausted by pump I2. Therefore it does not matter that filament 23 changes the composition of the gas by cracking because grid 2'? protects the instrument from any variation in measurements due to the same. Other irregularities in ionization of the gas, such as thermal cracking and formation of ions on the surface of the filament itself, make the complete removal of gas passing close to the filament essential in order to achieve a high degree of accuracy.

Example I The reading of milliammeter 53 will vary from instrument to instrument, the relative readings will be difierent for the different gases and about of the order set forth in the following table. This table is made at a constant pressure of 1G mm. of mercury. Obviously all comparative tests should be made at the same constant pressure, as varying the pressure varies the amount of ionization. This selected constant pressure can be chosen from a quite wide range of pressures, however, but preferably is chosen from the best range of operation, which runs from 10 mm. to 10- mm. of mercury, and I prefer the neighborhood of 10* mm. of mercury, as the best range to operate it. Once the pressure is selected it is maintained constant as closely as it is possible to It should be obvious that if only butene-l and butadiene are present in tube 4 a reading intermediate 2.60 and 1.26 will be given at milliammeter 53. By tests of known amounts of these gases a calibration table can be prepared from which the reading can be translated into definite percentages of each component. Other similar uses are obvious with more than two gases where only one gas varies. Other uses are suggested to those skilled in the art by this example.

While I have shown and described a certain arrangement of parts for carrying out the process of my invention and have described certain specific processes, these have been for purpose of illustration and obviously my invention is not limited thereto but instead is as defined in the following claims.

Having described my invention, I claim:

1. In a device of. the character described an evacuated chamber, and means to regulate the pressure in said chamber comprising vacuum pump means for evacuating said chamber to a predetermined pressure, and means supplying gas to maintain said pressure comprising a source of said gas at greater than atmospheric pressure, a conduit connecting said source and said chamber, a constant pressure regulating valve in said conduit receiving gas from said source and passing it under reduced pressure through said conduit, a pair of cut-off valves in said conduit downstream of said regulating valve, means to open and close said cut-off valves in order whereby that portion of said conduit between them acts as a metering chamber, a pressure equalizing chamber connected to said conduit downstream of said last cut-off valve, and a restricted orifice controlling flow from said conduit into said evacuated chamber.

2. In a device of the character described an evacuated chamber, and means to regulate the pressure in said chamber comprising vacuum means for evacuating said chamber to a predetermined pressure, and means supplying gas to maintain said pressure comprising a source of said gas, a conduit connecting said source and said chamber, a pressure regulating valve in said conduit receiving gas from said source and passing it under reduced pressure through said conduit, a pair of cut-off valves in said conduit downstream of said regulating valve, means to open and close said cut-01f valves in order whereby that portion of said conduit between them acts as a metering chamber, a pressure equalizing chamber connected to said conduit downstream of said last cut-off valve, and a restricted. orifice controlling flow from said conduit into said evacuated chamber.

3. In a device of the character described an evacuated chamber, and means to regulate the pressure in said chamber comprising vacuum pump means for evacuating said chamber to a predetermined pressure, and means supplying gas to maintain said pressure comprising a source of said gas, conduit connecting said source and said chamber, a constant pressure regulating valve in said conduit receiving gas from said source and passing it under reduced pressure through said conduit, a pair of cut-off valves in said conduit downstream of said regulating valve, means to open and close said cut-off valves in order whereby that portion of said conduit between them acts as a metering chamber, a pressure equalizing chamber connected to said conduit downstream of said last cut-off valve, and a restricted orifice controlling flow from said conduit into said evacuated chamber.

4. In a device of the character described an evacuated chamber, and means to regulate the pressure in said chamber comprising vacuum pump means for evacuating said chamber to a predetermined pressure, and means supplying gas to maintain said pressure comprising a source of said gas at greater than atmospheric pressure, a conduit connecting said source and said chamber, a constant pressure regulating valve in said conduit receiving gas from said source and passing it under reduced pressure through said conduit, a pair of cut-off valves in said conduit downstream of said regulating valve, means to open and close said cut-ofi valves in order whereby that portion of said conduit between them acts as a metering chamber, and a restricted orifice controlling flow from said conduit into said evacuated chamber.

5. In a device of the character described an evacuated chamber, and means to regulate the pressure in said chamber comprising vacuum means for evacuating said chamber to a predetermined pressure, and means supplying gas to maintain said pressure comprising a source of said gas, a conduit connecting said source and said chamber, a pressure regulating valve in said conduit receiving gas from said source and passing it under reduced pressure through said conduit, a pair of cut-off valves in said conduit downstream of said regulating valve, means to open and close said cut-ofi valves in order whereby that portion of said conduit between them acts as a metering chamber, a pressure equalizing chamber connected to said conduit downstream of said last cut-ofi valve, and a restricted orifice controlling flow from said conduit into said evacuated chamher.

6. The process of regulating the pressure in a chamber comprising the steps of evacuating said chamber to a predetermined pressure, supplying a gas to maintain said pressure from a source of said gas at a greater than atmospheric pressure by regulating the gas coming from said source to a constant pressure, metering said gas under constant pressure into a metering zone, passing said metered gas into a pressure equalizing zone and equalizing the pressure therein, and diffusing said gas from said equalizing zone through a restricted orifice into said chamber.

7. In a device of the character described an evacuated chamber, and means to regulate the pressure in said chamber comprising vacuum means for evacuating said chamber to a predetermined pressure, and means supplying gas to maintain said pressure comprising a constant pressure source of said gas, a conduit connecting said source and said chamber, a pair of cut-01f valves in said conduit, means to open and close said cut-off valves in order whereby that portion of said conduit between them acts as a metering chamber, a pressure equalizing chamber connected to said conduit downstream of said last cut-off valve, and a restricted orifice controlling flow from said conduit into said evacuated chamher.

8. The process of regulating the pressure in a chamber comprising the steps of evacuating said chamber to a predetermined pressure, supplying a gas to maintain said pressure from a source of said gas at constant pressure, metering discrete volumes of said gas under constant pressure into a metering zone, passing said metered gas into a pressure equalizing zone and equalizing the pressure therein, and diffusing said gas from said equalizing zone through a restricted orifice into said chamber.

THOMAS D. MORGAN.

References Cited in the file of this patent UNITED STATES PATENTS Number 

